Quantitative analysis of electrodeposited tin film morphologies by atomic force microscopy

This study of the electrodeposition of tin on steel substrates demonstrates that it is possible to obtain quantitative information on the thin film growth at industrially relevant substrates using atomic force microscopy (AFM) to monitor the film morphology and X-ray fluorescence (XRF) to measure the average film thickness. The effects of current density and electrolyte temperature on the film morphology, surface roughness, and grain size distribution (GSD) are reported. While the roughness of the substrates used in this study can vary by several hundred nanometers to a micrometer, we are interested in quantitative characterization of the tin films with thickness varying from a few tens of nanometers to several hundred nanometers. This study shows that for the range of film thickness and length scale studied, analysis of the AFM images can provide quantitative characterization of the thin film roughness and grain size distribution at various stages of growth with little interference from the substrate morphological inhomogeneities.     

利用线性酚醛树脂制备有序介孔碳

三嵌段共聚物F127为模板剂,线性酚醛树脂为碳前驱体,采用溶剂挥发诱导有机-有机自组装法(EI-SA)制备了具有二维六方结构的有序介孔碳。利用FT-IR、XRD、TEM、N2吸附/脱附等方法对有序介孔碳的结构进行了表征,研究了不同焙烧温度和模板剂用量对有序介孔碳结构的影响。结果表明,当模板剂的用量一定时,有序介孔碳的孔径、孔容和孔壁厚度都随着焙烧温度的升高而降低,但比表面积却随着微孔含量的增加而增大。随着模板剂用量的增加,介孔碳的有序性降低。有序介孔碳PF-2-500的比表面积、孔径、孔容、孔壁厚度和微孔比表面积比分别为583.82m2/g、3.05nm、0.31cm3/g、3.40nm和361.18m2/g,而有序介孔碳PF-1-500的比表面积、孔径和孔容相对于PF-2-500有所提高,分别为647.79m2/g、3.44nm和0.41cm3/g,但微孔比表面积和孔壁厚度分别降低为309.46m2/g和3.35nm。     

Direct transfer patterning of gold films with minimal processing steps

We were able to reduce the processing steps of transfer printing of thin gold films through prolonged evaporation times. We suspect the reduced evaporation rate to cause diffusion of small chain molecules (oligomers) in the PDMS (poly(dimethylsiloxane)) stamp to facilitate the transfer. Typical wrinkling of the PDMS surface was avoided by fabricating thin stamps of approximately 50 μm with polymer backing. The transferred films with a thickness of 20 nm showed enhanced edge resolution and a roughness of 1.31 nm root mean square. We were further able to fabricate 3D structures, indicating stability of the transferred films. Adhesion problems remain a limitation for contacting purposes.     

Characterization of the surface of bio-ceramic thin films

The biocompatibility and corrosion resistance of orthopaedic and dental implants are determined by their material composition and surface microstructural properties such as surface roughness, grain size, etc. Thin films of bio-inert materials such as oxides of Ti, Al, Zr, and bio-active materials such as hydroxy-apatite (Ca₁₀(PO₄)₆(OH)₂), compounds of calcium and phosphorous oxides are more attractive as bio-ceramic films because of their biocompatibility being higher, and toxicity being lower than those of the other materials. In this study, we mainly focused on characterization of the surface of bio-ceramics using atomic force microscopy (AFM). These films having a thickness of about 500 nm, had been processed using ion-beam sputter deposition, and ion-beam-assisted sputter deposition methods. Investigation of the surface of the films by AFM shows that irradiation with oxygen ions in the energy range of 3 keV increases the surface roughness. A detailed study of the grain size and roughness of several experimental cases of TiO₂ thin films showed that the films contained columnar grains with mean size of about 100 × 100 nm² grown in the z direction with a height of a few nanometers.     

Chemical solution approaches to YBa2Cu3O7_delta-Au nanocomposite superconducting thin films

We explore the feasibility of preparing YBa2CU3O7-Au (YBCO-Au) nanocomposite thin films by chemical solution deposition (CSD). Two approaches were used: (i) A standard in-situ methodology where Au metallorganic salts are added into the precursor solution of YBCO trifluoroacetate (TFA) salts and (ii) a novel approach where stable colloidal solutions of preformed gold nanoparticles (5-15 nm) were homogeneously mixed with TFA-YBCO solutions. A detailed analysis of the microstructure of the films showed that in both cases, there is a strong tendency of gold nanoparticles to migrate to the film surface. However the kinetics of this migration evidences important differences and in the case of preformed nanoparticles their size remains unchanged (a few nanometers) whereas for the in-situ nanocomposites gold ripening leads to large particles (hundreds of nanometers). The grown YBCO-Au films showed good superconducting characteristics (J(c) 2 MA/cm2 at 77 K) but the absence of Au inclusions inside the YBCO matrix explains the fact that no enhancement of vortex pinning was observed.     

Fabrication of gold micro- and nanostructures by photolithographic exposure of thiol-stabilized gold nanoparticles

Exposure of thiol-stabilized gold nanoparticles supported on silicon wafers to UV light leads to oxidation of the thiol molecules and coagulation of the nanoparticles, forming densified structures that are resistant to removal by solvent exposure. Unoxidized particles may, in contrast, readily be removed leaving gold structures behind at the surface. This process provides a convenient and simple route for the fabrication of gold structures with dimensions ranging from micrometers to nanometers. The use of masks enables micrometer-scale structures to be fabricated rapidly. Exposure of nanoparticles to light from a near-field scanning optical microscope (NSOM) leads to the formation of gold nanowires. The dimensions of these nanowires depend on the method of preparation of the film: for spin-cast films, a width of 200 nm was achieved. However, this was reduced significantly, to 60 nm, for Langmuir-Schaeffer films.     

New Triblock Copolymer Templates,PEO‐PB‐PEO,for the Synthesis of Titania Films with Controlled Mesopore Size,Wall Thickness,and Bimodal Porosity

The synthesis and properties of a series of new structure‐directing triblock copolymers with PEO‐PB‐PEO structure (PEO = poly(ethylene oxide) and PB = polybutadiene) and their application as superior pore‐templates for the preparation of mesoporous titania coatings are reported. Starting from either TiCl₄ or from preformed TiO₂ nanocrystalline building blocks, mesoporous crystalline titanium oxide films with a significant degree of mesoscopic ordered pores are derived, and the pore size can be controlled by the molecular mass of the template polymer. Moreover, the triblock copolymers form stable micelles already at very low concentration, i.e., prior to solvent evaporation during the evaporation‐induced self‐assembly process (EISA). Consequently, the thickness of pore walls can be controlled independently of pore size by changing the polymer‐to‐precursor ratio. Thus, unprecedented control of wall thickness in the structure of mesoporous oxide coatings is achieved. In addition, the micelle formation of the new template polymers is sufficiently distinct from that of typical commercial PPO‐PEO‐PPO polymers (Pluronics; PPO = poly(propylene oxide)), so that a combination of both polymers facilitates bimodal porosity via dual micelle templating.     

Morphology and electrical resistance of thin gold films on air-cleaved potassium chloride surfaces

The structures of vacuum-evaporated thin gold films on air-cleaved KCl single-crystal surfaces were studied by transmission electron microscopy and electrical resistance measurements. Preferential growth of gold crystallites along the cleavage steps was observed and confirmed by the presence of one-dimensional conduction. Films of average thickness 1.5 nm or less showed an island structure and did not exhibit electrical conduction. Films with thickness of 2.0 nm and 2.5 nm had network structures and displayed one-dimensional conduction along the steps and two-dimensional conduction on the surface respectively. The electrical resistance was not stable for the 2.0 nm film, while the 2.5 nm film had stable values. The resistance of films of average thickness 2.0 and 2.5 nm decreased as the temperature decreased but the effect was small.     

Preparation of 3-dimensional SiO2 structures via a templating method

Three-dimensional (3D) SiO₂ has been prepared by coating silica on the surface of a template polymer and a sequent calcination of the silica/polymer composite. The template polymer that has 3D skeletal structure was prepared by curing epoxy resin in polyethylene glycol mediums using diethylenetriamine as a curing agent. The coating of silica on the polymer surface was accomplished through a slow in situ hydrolysis of infiltrated ethyl silicate in the interconnected pore network of the template polymer. The thickness of silica layer was controlled in a range of 20-80 nm by changing the total amount of ethyl silicate in hydrolysis. The 3D structures of silica were characterized by scanning electronic microscopy, transmitting electronic microscopy, Fourier transform infrared spectroscopy and surface area measurement. The light scattering of the 3D silica filled with liquid medium can be minimized by tuning the refractive index of the liquid medium to be the same as that of amorphous silica in the 3D structure.     

Analysis of optical surfaces by means of surface plasmonspectroscopy

The sensitivity to material parameters of surface plasmon oscillations is explored for the design of a prototype system operating at a wavelength of 670 nm, for the simultaneous determination of thickness, complex permittivity and surface roughness of metal films. The apparatus was employed for characterization of gold and silver films with thicknesses within the 10-100 nm range. Thickness data measured with the prototype system were well correlated with those measured on a conventional surface profilometer. The Fourier spectrum of surface irregularities extracted from scattered light, enhanced by surface plasmon oscillations, was used to determine surface roughness parameters for the distinct samples. Those parameters were shown to be representative of typical surface structures observed with the atomic force microscope     

Ellipsometric characterization of SiOx films with embedded Si nanoparticles

In this work we present results on the ellipsometric study of SiO_x films in the spectral range of 280-820 nm. The films were deposited by vacuum thermal evaporation of SiO onto Si substrates heated at 150 °C. To stimulate the formation of silicon clusters in the oxide matrix the films were annealed at temperatures 700, 1000 and 1100 °C in argon for 5, 15 and 30 min. By applying the Bruggeman effective-medium approximation theory and using multiple-layer optical models, from the ellipsometric data analysis the thickness, complex refractive index and composition of the films, as well as the size of the embedded Si nanocrystallites have been determined. Atomic-force microscopy imaging showed a very smooth surface, the roughness value of which correlated well with the top-layer thickness, determined from the ellipsometric data analysis.     

Thermal Effusivity Determination of Metallic Films of Nanometric Thickness by the Electrical Micropulse Method

The thermal effusivity of gold, aluminum, and copper thin films of nanometric thickness (20 nm to 200 nm) was investigated in terms of the films’ thickness. The metallic thin films were deposited onto glass substrates by thermal evaporation, and the thermal effusivity was estimated by using experimental parameters such as the specific heat, thermal conductivity, and thermal diffusivity values obtained at room conditions. The specific heat, thermal conductivity, and thermal diffusivity values of the metallic thin films are determined with a methodology based on the behavior of the thermal profiles of the films when electrical pulses of few microseconds are applied at room conditions. For all the investigated materials, the thermal effusivity decreases with decreased thickness. The thermal effusivity values estimated by the presented methodology are consistent with other reported values obtained under vacuum conditions and more elaborated methodologies.     

Influence of substrate rotation speed on the nanostructure of sculptured Cu thin films

Different rotation speeds of the substrate about its surface normal were used to produce sculptured copper thin films of ∼ 90 nm thickness. X-ray diffraction (XRD), atomic force microscopy (AFM) and scanning electron microscopy (SEM) were employed to obtain nano-structure and morphology of these films. Their optical properties were measured by spectrophotometry in the spectral range of 340-850 nm. Real and imaginary refractive indices, film thickness and fraction of metal inclusion in the film structure were obtained from optical fitting of the spectrophotometer data.     

Phase separation and surface morphology of spin-coated films of polyetherimide/polycaprolactone immiscible polymer blends

The surface morphology in thin films of immiscible polyetherimide and polycaprolactone blends was studied using scanning electron and atomic force microscopy. The thin films were obtained by spin-coating from dichloromethane solution. A self-assembled periodic pattern of phase separated domains was observed, which was induced by capillary effects along with the solution radial flow and the unsteady air flow field above the film during the initial stages of spin-coating. A secondary phase separation was observed during the solvent evaporation stage of spin-coating. The differences in surface topographies of the two distinct phases are attributed to different solvent evaporation rates within each phase. In addition, a great variety of domain structures and surface morphologies were observed as a function of polymer blend composition.     

Dynamic scale theory for characterizing surface morphology of layer-by-layer films of poly(o-methoxyaniline)

The dynamic scale theory and fractal concepts are employed in the characterization of surface morphological properties of layer-by-layer (LBL) films from poly(o-methoxyaniline) (POMA) alternated with poly(vinyl sulfonic acid) (PVS). The fractal dimensions are found to depend on the procedures to fabricate the POMA/PVS multilayers, particularly with regard to the drying procedures. LBL films obtained via drying in ambient air show a more homogeneous surface, compared to films dried under vacuum or a flow of nitrogen, due to a uniform rearrangement of polymer molecules during solvent evaporation.     

On morphological, structural and electrical properties of vacuum deposited pentacene thin films

Films of different thickness (50, 100, 150 and 200 nm) were deposited by thermal evaporation in vacuum on two types of substrates glass and ITO. The deposition was performed under a pressure of 10⁻⁶ mB with a rate of 0.25 nm/s. Films surface investigations showed morphological and structural changes in function of films thickness and the nature of the substrate. Films optical transmission was analysed in the 280-1600 nm spectral range and the electrical measurements were done in low vacuum (10⁻¹:10⁻² mB) and in dark.     

Fabrication of a nickel nanowire mesh electrode suspended on polymer substrate

We report on an efficient strategy for the fabrication of an ultra-long suspended nanowire mesh suitable for nanodevice architectures on a polymer surface. First, nickel nanowires are synthesized directly on a template substrate by magnetron sputtering. Laser interference lithography followed by deep reactive ion etching is used to create the nanograted template substrate constituted of one-dimensional line pattern arrays of 240 nm in periodicity. Ordered alignment of ultra-long nanowires (～180 nm in diameter) with high fidelity to the template pattern is observed by scanning electron microscopy. The transfer of the pre-defined parallel nanowire array from the template surface to a target polymer substrate for electrical characterization of the system is demonstrated. The electrical behaviour of the nanowire mesh, suspended between two electrodes, was found to be linear, stable, and reproducible. This result suggests that this nanofabrication process will open an efficient way to the design and construction of novel nanodevices.     

Thin film passive solar windows produced by reactive evaporation of In-Sn

The semiconductor indium tin oxide (ITO) when present as a thin film has been shown to be transparent to visible radiation while opaque to IR radiation. Sputtering, chemical vapor deposition and other coating methodologies have been used to prepare ITO thin films. Reactive evaporation is an alternative coating technique, which has as its major advantage technical simplicity. Our prepation of ITO thin films (30–90 nm) for passive solar windows included the reactive evaporation of In-Sn alloys (In-5wt.%Sn, In-10wt.%Sn and In-20wt.%Sn) onto commercial soda-lime glass held between 25 and 300 °C. The reactive evaporation atmosphere consisted of oxygen at partial pressures from 1 × 10^-4 to 1 × 10^-3 Torr in residual nitrogen. In selected instances ultrathin palladium nucleating layers were evaporated onto the glass substrates prior to the deposition of the ITO. This was done in order to minimize initial alloy-glass agglomeration effects, thus decreasing the final overall ITO film thickness while increasing the visible transmission properties. The film's visible and IR spectral transmission properties were examined using ratio recording spectrophotometry. The agglomeration, nucleation and growth phenomena of the films were extensively investigated by transmission electron microscopy. The agglomeration was found to be a function of the film thickness, with increasing agglomeration for thinner films. Surface analysis by scanning Auger microscopy (SAM), electron spectroscopy for chemical analysis (ESCA), scanning electron microscopy and energy-dispersive analysis of X-rays was also extensively carried out to determine our particular film properties. SAM indicated that only indium, tin and oxygen were present. No tungsten from the evaporation filament or elements from the glass were found. ESCA indicated that ITO was indeed present on the surface. Such work definitely indicated that ITO can be prepared by reactive physical vapor deposition and that the resultant films have the properties commonly found in sputtered ITO films.     

苯乙烯-马来酸酐共聚物/金纳米微粒的合成

以氯金酸为原料,DMF(N,N-二甲基甲酰胺)为溶剂及还原剂,苯乙烯-马来酸酐共聚物为大分子稳定剂,合成了金纳米微粒。通过紫外-可见吸收光谱、透射电子显微镜等方法对纳米金样品进行了表征。结果表明:所得到的金纳米微粒可以在520 nm~530 nm范围内产生明显的纳米金所具有的特征等离子共振吸收峰,金纳米微粒的尺寸在3 nm~5nm且具有较窄的分布,证明苯乙烯-马来酸酐共聚物可以对金纳米微粒表面产生较好的修饰作用,从而为制备纳米金材料提供了一种新的途径。